Fabrication and sub-band-gap absorption of single-crystal Si supersaturated with Se by pulsed laser mixing

Selenium supersaturated silicon layers were fabricated by pulsed excimer laser induced liquid-phase mixing of thin Se films on Si(001) wafers. Sufficiently low Se coverage avoids destabilization of rapid epitaxial solidification, resulting in supersaturated solid solutions free of extended defects, as shown by transmission electron microscopy. The amount of retained Se depends on the original film thickness, the laser fluence, and the number of laser pulses irradiating the same spot on the surface. Using this method, Se has incorporated into the topmost 300 nm of the silicon with a concentration of 0.1 at.%. Channeling Rutherford backscattering spectrometry measurements show that the substitutional fraction can be as high as 75% of the total retained Se. These alloys exhibit strong sub-band-gap absorption with optical absorption coefficient ranging up to about 10⁴ cm⁻¹, thus making them potential candidates for applications in Si-based optoelectronic devices.     

Template-directed hydrothermal synthesis of hydroxyapatite as a drug delivery system for the poorly water-soluble drug carvedilol

In order to improve the dissolution rate and increase the bioavailability of a poorly water-soluble drug, intended to be administered orally, the biocompatible and bioactive mesoporous hydroxyapatite (HA) was successfully synthesized. In the present study, mesoporous HA nanoparticles were produced using Pluronic block co-polymer F127 and cetyltrimethylammonium bromide (CTAB) as templates by the hydrothermal method. The obtained mesoporous HA was employed as a drug delivery carrier to investigate the drug storage/release properties using carvedilol (CAR) as a model drug. Characterizations of the raw CAR powder, mesoporous HA and CAR-loaded HA were carried out by the scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray powder diffraction (XRPD), differential scanning calorimetry (DSC), Fourier transform infrared (FT-IR) spectroscopy, N₂ adsorption/desorption, thermogravimetric analysis (TGA), and UV-VIS spectrophotometry. The results demonstrated that CAR was successfully incorporated into the mesoporous HA host. In vitro drug release studies showed that mesoporous HA had a high drug load efficiency and provided immediate release of CAR compared with micronized raw drug in simulated gastric fluid (pH 1.2) and intestinal fluid (pH 6.8). Consequently, mesoporous HA is a good candidate as a drug carrier for the oral delivery of poorly water-soluble drugs.     

光电检测法在线测控糖液过饱和度的研究

过饱和度是糖液结晶过程中的主要测控参量.本文报道一种新型的光电检测法在线测控糖液过饱和度的原理与方法,给出其理论模型、系统构成和在单晶冰糖结晶工序上的应用结果.     

Enhanced gastrointestinal absorption of N3-O-toluyl-fluorouracil by cationic solid lipid nanoparticles

This study was aimed to prepare N₃-O-toluyl-fluorouracil (TFu) loaded cationic solid lipid nanoparticles (TFu-SLNs) and evaluate the potential of a novel lipid-based drug delivery system to enhance the oral absorption of TFu. TFu-SLNs were prepared by the film dispersion-ultrasonication method, using hexadecyltrimethylammonium bromide as cationic tenside. The formulation and manufacture parameters were optimized concerning the drug encapsulation efficiency and the particle size. The in vitro release characteristics, in vivo pharmacokinetic properties and bioavailability, and in situ intestinal absorption features were investigated. The morphology of TFu-SLNs was approximately spherical and the mean particle size was 178.8 ± 9.99 nm; the zeta potential was +19.54 ± 0.32 mV. The mean entrapment efficiency and drug loading were 71.03 ± 1.19% and 3.57 ± 0.08%, respectively. The release behaviors of TFu from TFu-SLNs in PBS were fitted to the bioexponential model, while in artificial gastric juice, artificial intestinal juice and artificial gastric juice (2 h) followed by artificial intestinal juice (2–48 h) were fitted to the Weibull equation. The results of the pharmacokinetic studies in mice showed that the bioavailability of TFu-SLNs was significantly increased compared with that of the TFu suspensions after oral administration. The absorption of TFu-SLNs in intestine of rat was fitted to first-order kinetics with passive diffusion mechanism and the main segments of TFu-SLNs absorbed in intestine were duodenum and jejunum for the bioadhesion mediated by electrostatic interaction between the positively charged colloidal particles and the negatively charged mucosal surface. These results indicated that cationic SLNs would offer a promising delivery system for the facilitation of the bioavailability of poorly oral absorption drugs by enhancing the bioadhesion between the absorption mucosal surface and the drug carriers.     

急冷Ag-Ge二元系合金的相关系

用X射线衍射和热学分析的方法研究了急冷(冷却速度约为10⁴K/s)Ag-Ge二元系样品的相关系。由于急冷Ge在Ag中的溶解度由平衡下的1.5at％扩展到8at％。在Ge含量为8—23at％的样品中,除含Ge在Ag中的过饱和固溶体和Ge外,还有一个具有与Ag基过饱和固溶体相同成分,不同堆垛形式的亚稳相,属A3型六角密排结构,点阵常数a=2.893±0.010?,c=4.720±0.010?,c/a=1.632。用DuPont公司1090系列的差示扫描量热仪(DSC)研究了过饱和固溶体和 关键词：     

Formation of nanosize Li-ferrites from acetylacetonato complexes and their crystal structure, microstructure and order–disorder phase transition

Nanosize Li-ferrites were synthesised by the thermal decomposition of an appropriate mixture of complex compounds with acetylacetone - (2,4 pentadione) ligands ([M(AA)_x]; M=Li and Fe) at 500 °C. The obtained sample is composed of three phases determined by the standard Rietveld procedure: Li_0.5Fe_2.5O₄ (S.G. P4₃32), Li_1.16Fe₃O₄ (S.G. Fd 3̄ m) and LiFeO₂ (S.G. Fm 3̄ m). Cation distribution in nanosize ordered spinel Li_0.5Fe_2.5O₄ deviates from that of the bulk counterpart. Microstructure parameters (crystallite size of ∼23 nm and strain of 3.2526(9)×10³) were determined by the Rietveld refinement of the TCH-pV parameters. SEM microphotographs show a particle size of ∼50–60 nm. An order–disorder phase transition in ordered spinel Li_0.5Fe_2.5O₄was studied by DSC measurements and in situ XRPD technique.The temperature of phase transition was found to be 762 °C (DSC) and (±) 7455°C.(XRPD)PACS 81.07.Bc; 81.16.Be; 61.66.Fn; 61.50.Ks     

Dopant activation in Sb-implanted relaxed Si1−xGex alloy layers grown on compositionally graded buffers

Supersaturated solid solutions of substitutional, electrically active Sb have been obtained by ion implantation of relaxed epitaxial Si_1?xGe_x alloy layers grown on compositionally graded buffers. Substitutional and nonsubstitutional Sb fractions in relaxed Si_0.85Ge_0.15, Si_0.65Ge_0.35 and Si_0.50Ge_0.50 alloy layers implanted to a dose of 5×10¹⁵ Sb cm^?2 and annealed isothermally at temperatures ranging from 400 to 850°C have been studied by Rutherford backscattering/channeling, transmission electron microscopy and Hall-effect and sheet resistivity measurements. A supersaturated solution of Sb corresponding to a peak carrier concentration of 4×10²⁰ cm^?3 and an electrically active fraction of 40% of the implanted dose is observed by Hall measurements for the case of Si_0.85Ge_0.15 and Si_0.65Ge_0.35 alloys annealed at 550°C.     

An attempt at kidney stone analysis with the application of synchrotron radiation

X‐ray absorption near‐edge spectroscopy (XANES) is a spectroscopic technique using synchrotron light to determine the valence state of excited atoms as well as the electronegativity of their neighbouring atoms. XANES spectra can provide information about the chemical bond in the second coordination shell of the excited atom. In this study, XANES spectra of unknown compounds from human kidney stones were recorded around the K‐edges of sulfur, phosphorus and calcium. The XANES results agree well with the diffractogram data of the same stones obtained through an X‐ray powder diffraction (XRPD) technique. By comparing the measurement techniques presented here, it is shown that XANES requires a smaller amount of each sample than XRPD for analysis.     

Preparation and Characterization of Novel Polyimides with Hydroxyl Groups

3,3′-diamino-4,4′-dihydroxybiphenyl (DADHBP) was synthesized and its chemical structure was confirmed by Fourier transform infrared (FT-IR) spectroscopy, ¹H-nuclear magnetic resonance (¹H-NMR), and differential scanning calorimetry (DSC). Then six poly(amic acid) (PAA) solutions were prepared by copolymerization of DADHBP, oxydiphthalicanhydride (ODPA), and 2,2-bis [4-(4-aminophenoxy)phenyl] propane (BAPOPP) in N,N-dimethylacetamide (DMAC) in different mole ratios. The polyimide (PI) films were obtained through thermal imidazation reactions of the thin layers of the above-mentioned precursor solutions. Chemical structures of all PI films were demonstrated by FT-IR. Thermal stabilities and decomposition behaviors of the PI films were tested by DSC and thermogravimetric analysis (TGA). Thermal measurements indicate that the polymers have high thermal stability and produce high char yields. The properties of the PI films were further studied by ultraviolet–visible spectroscopy, water absorption, surface energy, and mechanical measurements. Thermal analysis showed glass transition temperatures between 205.9°C and 276.7°C. Decomposition temperatures were higher than 360.2°C, with 10% weight losses in the range of 448.6°C～517.8°C. The prepared PI films also exhibited good UV absorption, low water absorption (<2%), low surface energy (<44.28 mJ/m²), and good mechanical properties.     

Tetramethylpolyarylate-polyarylate block copolymer: Synthesis and miscibility with polyarylate and poly(styrene-co-acrylonitrile)

Abstract

Tetramethylpolyarylate-polyarylate (TMPAr-PAr) block copolymers of various block lengths were synthesized by the coupling reaction of hydroxy-terminated TMPAr and hydroxy-terminated PAr using triphosgene. The phase behavior of these block copolymers are discussed based on the thermal properties observed by differential scanning calorimetry (DSC). The thermal properties of binary blends of these block copolymers with PAr homopolymer or poly(styrene-co-acrylonitrile) whose acrylonitrile content is 9.5 wt% (SAN 10) were observed by DSC. The compatibilizing effect of the microphase-separated TMPAr-PAr block copolymer in PAr/SAN 10 blends was observed from thermal properties and morphology.     

Homogeneous Cu–Fe supersaturated solid solutions prepared by severe plastic deformation

A Cu–Fe nanocomposite containing 50 nm thick iron filaments dispersed in a copper matrix was processed by torsion under high pressure at various strain rates and temperatures. The resulting nanostructures were characterized by transmission electron microscopy, atom probe tomography (APT) and Mössbauer spectrometry. It is shown that α-Fe filaments are dissolved during severe plastic deformation leading to the formation of a homogeneous supersaturated solid solution of about 12 at% Fe in fcc Cu. The dissolution rate is proportional to the total plastic strain but is not very sensitive to strain rate. Similar results were found for samples processed at liquid nitrogen temperature. APT data revealed asymmetric composition gradients resulting from deformation-induced intermixing. On the basis of these experimental data, the formation of the supersaturated solid solutions is discussed.     

Supersaturated Si-As alloy formation by ion implantation and pulsed electron beam annealing

Supersaturated surface alloys produced by very high dose (0.8–2.6×10¹⁷cm^–2) implantation of As-ions into silicon and subsequent pulsed electron-beam annealing have been investigated by means of the channeling technique. The maximum solubility limit of 7×10²¹ As/cm³ has been determined. It exceeds the equilibrium solubility limit by more than a factor of 4. Angular scan measurements indicated that for doses above 1×10¹⁷cm^–2 As atoms are displaced by about 0.12 Å from the regular lattice sites.     

High Pressure X-Ray Absorption and Diffraction Study of InAs

We have performed X-ray absorption (XAS) and diffraction (XRD) measurements at high pressure on samples of powdered InAs, up to 50 and 80 GPa, respectively. In the lower pressure range, our data are consistent with the following structural sequence: Zincblende M NaCl M Cmcm . The first order transition from the semiconducting Zincblende phase to the metallic NaCl phase is clearly seen by the shift in the absorption onset at the As K-edge and the strong modifications of the extended X-ray absorption fine structure (EXAFS) due to the changes in the local structure from a 4-fold to a 6-fold coordinated environment. XAS shows the high pressure phase to be locally site-ordered. The diffraction data, analized by Rietveld fitting, gives a volume discontinuity of j V/V 0 ～0.18 for the first order transition. There is no apparent volume discontinuity associated to the NaCl M Cmcm transition.     

Polychrome glass from Etruscan sites: first non-destructive characterization with synchrotron μ-XRF, μ-XANES and XRPD

This work is devoted to the characterization of a suite of very rare, highly decorated and coloured glass vessels and beads from the VII to the IV century BC. The most serious difficulty in developing this study was that any sampling – even micro-sampling – was absolutely forbidden. As a consequence, the mineralogical and chemical nature of chromophores and opacifiers present in these Iron Age finds were identified by means of the following synchrotron-based, strictly non-destructive, techniques: micro X-ray fluorescence (μ-XRF), Fe K-edge micro X-ray absorption near edge spectroscopy (μ-XANES) and X-ray powder diffraction (XRPD). The μ-XRF mapping evidenced high levels of Pb and Sb in the yellow decorations and the presence of only Sb in the white and light-blue ones. Purple and black glass show high amounts of Mn and Fe, respectively. The XRPD analyses confirmed the presence of lead and calcium antimonates in yellow, turquoise and white decorations. Fe K-edge μ-XANES spectra were collected in different coloured parts of the finds, thus enabling the mapping of the oxidation state of these elements across the samples. In most of the samples iron is present in the reduced form Fe²⁺ in the bulk glass of the vessels, and in the oxidized form Fe³⁺ in the decorations, indicating that these glass artefacts were produced in at least two distinct processing steps under different furnace conditions. PACS  29.20.Lq; 81.80.Kf; 61.10.Ht     

Copper (50 MeV) and Oxygen (84 MeV) Ion Irradiation Probed Thermal,Structural and Optical Behavior of Polyethylene Terephthalate

Polyethylene terephthalate (PET) films of 50?μm thickness were exposed to swift-heavy 50?MeV copper and 84?MeV oxygen ions, with fluence varying from 1?×?10¹¹ to 1?×?10¹³ ions cm^?2. Differential scanning calorimetry (DSC), X-ray diffraction (XRD) and Fourier-transform infrared (FTIR) and UV-visible spectroscopic techniques were used to characterize the irradiated samples. The XRD and DSC analysis indicated the loss of crystallinity during/after the irradiation. The FTIR spectra revealed the formation of alkyne end groups, C═C groups and structural deformation with increase of ion fluence. Considerable reduction in the value of the optical bandgap was inferred from the study of the UV-visible absorption curves.     

Evaluation of an oral carrier system in rats: bioavailability and gastrointestinal absorption properties of curcumin encapsulated PBCA nanoparticles

A new oral delivery system, polybutylcyanoacrylate nanoparticles (PBCNs), was introduced to improve the oral bioavailability of curcumin (CUR), a poorly soluble drug. The formulation was optimized by orthogonal design and the optimal PBCNs loading CUR exhibited a spherical shape under transmission electron microscopy with a range of 40?C400?nm. Physicochemical state of CUR in PBCN was investigated by X-ray diffraction and the possible structure changes occurring in CUR after conjugating with polybutylcyanoacrylate were studied with FTIR. The results indicated that CUR in PBCN was in a non-crystalline state and CUR was encapsulated in PBCN without chemical reaction. The oral pharmacokinetic study was conducted in rats and the relative bioavailability of CUR encapsulated PBCNs to the crude CUR was more than 800%. The in situ absorption experiment in rat intestine indicated the absorption was first order with passive diffusion mechanism. The absorption results in various segments of intestine showed that the main absorption sites were ileum and colon. It can be concluded that PBCNs as an oral carrier can significantly improve the oral absorption of a poorly soluble drug.     

Sonochemical synthesis of supersaturated Ga–Al liquid-alloy fine particles and Al3+-doped γ-Ga2O3 nanoparticles by direct oxidation at near room temperature

In this study, we investigated the fabrication of supersaturated gallium (Ga)–aluminum (Al) liquid alloy and Al³⁺-doped γ-Ga₂O₃ nanoparticles (NPs) at near room temperature (60 °C) using sonochemical and sonophysical effects. Supersaturated Ga–Al liquid alloy microparticles (D_av = 1.72 µm) were formed and stabilized at 60 °C by the thermal nonequilibrium field provided by sonochemical hot spots. Compared with liquid Ga, supersaturated Ga–Al liquid alloy was rapidly oxidized to a uniform oxide without Al₂O₃ or Al deposition. Thus, ultrafine Al³⁺-doped γ-Ga₂O₃ NPs were obtained after only 1 h of ultrasonic irradiation at 60 °C. The oxidation of liquid Ga was remarkably accelerated by alloying with metallic Al and ultrasonic irradiation, and the time was shortened. The average diameter and surface area of the γ-Ga₂O₃-based NPs were 59 nm and 181 m²/g, respectively. Compared with γ-Ga₂O₃, the optical bandgap of the Al³⁺-doped γ-Ga₂O₃ NPs was broadened, and the thermal stability improved, indicating Al³⁺-doping into the γ-Ga₂O₃ lattice. However, the lattice constant of γ-Ga₂O₃ was almost unchanged with or without Al³⁺-doping. Al³⁺ was introduced into the defect sites of Ga³⁺, which were massively induced in the defective spinel structure during ultrasonic processing. Therefore, sonochemical processing, which provides nonequilibrium reaction fields, is suitable for the synthesis of supersaturated and metastable materials in metals and ceramics fields.     

Insight into microstructural development by XBroad program: Case of in-situ formation of the Al–Zn solid solution

Formation of the Al–15 at% Zn solid solution was followed by in-situ high-temperature X-ray powder diffraction (XRPD) measurements. It was found that the temperature of 200 °C marked an onset of the dissolution of Zn atoms in Al matrix, while the solid solution was formed at 300 °C. Change in the shape of Zn precipitates during the solid solution formation was analyzed by the XBroad program. The program provides adequate information about changes in size and/or transformation of shapes during different crystallization/dissolution processes without any prior information on structural features of the system under study. It was demonstrated that the XBroad program is an excellent tool for the quick and effective microstructural analysis easily used by material science community regardless of their background in the field of crystallography.     

Growth,structure, thermal,electrical and optical properties of potassium aluminum sulfate dodecahydrate (potash alum) single crystal

Single crystal of potassium aluminum sulfate dodecahydrate (potash alum) was grown by the slow evaporation technique of supersaturated aqueous solution at room temperature. The obtained crystal was characterized by using powder X-ray diffraction, DSC, TGA, electrical conductivity, optical transmittance and optical reflectance measurements. Structural and thermal analyses were performed on potash alum crystal. The electrical conductivity of potash alum as electrolyte sample was 1.894 × 10⁻⁶ S/cm. The optical transition and optical band gap energy of potash alum crystal were studied for the first time. Direct and indirect optical band gap energies were 5.75 and 4.50 eV respectively. Extinction coefficient, refractive index, real and imaginary dielectric constants and optical conductivity were calculated for potash alum crystal at a range of photon energies between 1.4 and 6.2 eV. Normal dispersion parameters of potash alum crystal were calculated for the first time.     

Cavity-ring-down spectroscopic studies of NO2 in the region around 613 nm

Catalytic degradation and diffusion processes of NO₂ were followed by cavity-ring-down spectroscopy (CRDS) at 612.9 nm. The suitability of this absorption method for quasi-continuous, direct quantitative measurements over extended periods of time is demonstrated. The high sensitivity of the method is reflected by the fact that NO₂ concentrations as low as 200 ppb were detected at wavelengths at which the absorption of NO₂ is 12-fold lower than at the absorption maximum at 413 nm. Absorption coefficients of less than 1×10^-7 cm^-1 were measured. Received: 25 February 2000 / Revised version: 4 August 2000 / Published online: 5 October 2000